节点文献
四苯基卟啉的催化合成和微波合成研究
SYNTHESIS OF MESOTETHAPHENYLPORPHYRINS\=(TPP) BY CATALYST IN SOLVENTS AND \=UNDER MICROWAVE IRRADATION
【摘要】 采用溶剂催化法和微波激励法合成meso-四苯基卟啉(TPP).发现所用溶剂的沸点和极性、催化剂的酸度(Pka)及反应体系中的水分含量是决定反应的主要因素.采用甲苯或二甲苯做溶剂,对硝基苯甲酸做催化剂,采用溶剂蒸除—填加同步法合成的四苯基卟啉产率达到58.4%.同样体系采用微波激励法,30min产率达到42%,反应速度提高了2.2倍.根据TPP与其主要副产物四苯基二氢卟啉(TPC)的紫外光谱特点以及分光光度法的加合性,采用双波长紫外光谱法测算产品纯度,测得重结晶纯化后产品纯度为97.7,柱色谱纯化后产品纯度达到99.76%.
【Abstract】 The synthetic methods of mesoPorphyrin(TPP) by solventcatalystreaction and under microwave irradation are explored in this paper. It was discoved that the boiling point and polarity of the solvents, acidity of the catalysts, and the content of water in the reaction system were the key factos. With pnitrobentoic acid as the catalyst in toluene or xylene and with a special solvent treatment of distilationaddition at same step, TPP was given by direct condensation of pyrrole and benzaldehyde to 58\^4% of the yield. Comparing with that, 42% of the yield of TPP was got under microwave irradation by the same reaction system in 30min, faster 4\^2 times that of reaction rate of the catalyst method. UV spectrum and cocomponentcalculation were used for valuing the product according to the great difference between the maximum adsorption in the UV spectrum of TPP and its main byproduct 2Hporphyrin(TPC). The purity of the product for TPP was 97\^7% and 99\^76% for recrystallization and column purilation respec
- 【文献出处】 北京轻工业学院学报 ,Journal of Beijing Institute of Light Indusry , 编辑部邮箱 ,1998年04期
- 【分类号】O626.13
- 【被引频次】134
- 【下载频次】518